CN111318721B - Preparation method of platinum nano-chain - Google Patents

Abstract

The invention discloses a preparation method of a platinum nano-chain, belongs to the technical field of preparation of platinum nano-materials, and aims to quickly synthesize the platinum nano-chain with the particle size of 3 nm. Which comprises the following steps: (1) soaking and cleaning a container required for preparing the platinum nano-chain with acid, and drying for later use; (2) adding 25mL of 0.01% chloroplatinic acid aqueous solution into a 100mL beaker, stirring and heating at 280 ℃ until boiling; (3) adding 500uL of 1% sodium citrate aqueous solution, 250uL of 0.1% sodium citrate aqueous solution and 250uL of 1% sodium borohydride aqueous solution into the chloroplatinic acid aqueous solution in sequence, immediately changing the solution from colorless to yellow brown, heating to boiling at 280 ℃, adjusting the temperature to 100 ℃ and continuously heating for 15min, changing the solution from yellow brown to light brown and not changing, removing a heat source, stirring for 10min, and cooling to room temperature; (4) and transferring the cooled solution into a 25mL volumetric flask, and performing constant volume to a scale by using ultrapure water to prepare a platinum nano-chain solution. The method is suitable for the preparation method of the platinum nano-chain.

Description

Preparation method of platinum nano-chain

Technical Field

The invention belongs to the technical field of preparation of platinum nano materials, and particularly relates to a preparation method of a platinum nano chain.

Background

The platinum nano material can not only reduce the platinum dosage by virtue of the special physical and chemical properties of the platinum nano material, but also has wide application prospects in the fields of catalysis, electrochemistry, thermology, medicine, biology and the like, so that the preparation of the platinum nano material has important significance.

At present, the preparation method of the platinum nano material mainly comprises an electrochemical method, a solvothermal method, a hydrothermal method, a microwave-assisted method and the like, and the prepared platinum nano material mainly comprises platinum nano particles, platinum nanowires and platinum nanorods. Through recent efforts, the synthesis of platinum nanomaterials has achieved some success, but morphology and size control of platinum nanomaterials remains a technical challenge facing this field.

Disclosure of Invention

The invention aims to: in order to solve the problems, a preparation method of the platinum nano-chain is provided, and the platinum nano-chain with the particle size of 3nm is rapidly synthesized.

The technical scheme adopted by the invention is as follows:

a preparation method of platinum nano-chains comprises the following steps:

(1) putting all glass containers required by the preparation of the platinum nanochain into aqua regia for soaking for 3 hours, then sequentially cleaning the glass containers by using tap water, deionized water and ultrapure water, and drying the glass containers for later use;

(2) adding 25mL of chloroplatinic acid aqueous solution with the mass fraction of 0.01% into a 100mL beaker, stirring and heating at 280 ℃ until the mixture is boiled;

(3) sequentially adding 500uL of 1 mass percent sodium citrate aqueous solution, 250uL of 0.1 mass percent sodium citrate aqueous solution and 250uL of 1 mass percent sodium borohydride aqueous solution into the chloroplatinic acid aqueous solution which is heated to boiling in the step (2), wherein at the moment, the solution is immediately changed from colorless to tawny, heating to boiling at 280 ℃, adjusting the temperature to 100 ℃ and continuously heating for 15min, the solution is changed from tawny to light brown and is not changed, removing a heat source, and then continuously stirring for 10min and cooling to room temperature;

(4) and (4) transferring the solution cooled to room temperature in the 100mL beaker in the step (3) to a 25mL volumetric flask, and carrying out constant volume to scale with ultrapure water to obtain the platinum nano-chain solution.

In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:

1. the method for preparing the platinum nano-chain solution has the advantages of simple operation, rapid preparation, low cost and the like; meanwhile, the prepared platinum nano-chain is of a chain structure with the particle size of 3nm, is polycrystalline and has a face-centered cubic structure.

2. In the invention, the temperature in step 3 is controlled at 280 ℃ to shorten the time for preparing the platinum nano-chain, but if the temperature is continuously 280 ℃, the solution volatilizes quickly, and agglomeration phenomenon is easy to occur, so that the preparation fails, and therefore, after the solution is heated to boiling at 280 ℃, the temperature needs to be adjusted to 100 ℃.

3. Repeatedly preparing the platinum nano-chain for many times according to the method of the invention, wherein the prepared platinum nano-chain keeps consistent; the ultraviolet-visible absorption spectrogram of the prepared platinum nano-chain has no obvious change within 90 days, and has good reproducibility and stability.

Drawings

FIG. 1 is a TEM representation of platinum nanochains of the present invention;

FIG. 2 is an electron diffraction pattern of platinum nanochains of the present invention;

FIG. 3 is a diagram of the ultraviolet-visible absorption spectrum of chloroplatinic acid and platinum nanochain solution in accordance with the present invention;

FIG. 4 is a diagram of the UV-VIS absorption spectra of the platinum nanochain solution of the present invention after being left for different periods of time.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

A preparation method of platinum nano-chains comprises the following steps:

(1) putting all glass containers required by the preparation of the platinum nanochain into aqua regia for soaking for 3 hours, then sequentially cleaning the glass containers by using tap water, deionized water and ultrapure water, and drying the glass containers for later use;

(2) adding 25mL of chloroplatinic acid aqueous solution with the mass fraction of 0.01% into a 100mL beaker, stirring and heating at 280 ℃ until the mixture is boiled;

(3) sequentially adding 500uL of 1 mass percent sodium citrate aqueous solution, 250uL of 0.1 mass percent sodium citrate aqueous solution and 250uL of 1 mass percent sodium borohydride aqueous solution into the chloroplatinic acid aqueous solution which is heated to boiling in the step (2), wherein at the moment, the solution is immediately changed from colorless to tawny, heating to boiling at 280 ℃, adjusting the temperature to 100 ℃ and continuously heating for 15min, the solution is changed from tawny to light brown and is not changed, removing a heat source, and then continuously stirring for 10min and cooling to room temperature;

(4) and (4) transferring the solution cooled to room temperature in the 100mL beaker in the step (3) to a 25mL volumetric flask, and carrying out constant volume to scale with ultrapure water to obtain the platinum nano-chain solution.

In the invention, the prepared platinum is a chain structure with the diameter of 3nm by combining with the attached figure 1. With reference to fig. 2, the diameters of the circular rings are 9.2951/nm, 10.8081/nm, 15.2761/nm and 17.8761/nm from inside to outside, the distances di of the crystal planes are calculated to be 0.230nm, 0.198nm, 0.140nm and 0.120nm (the camera constant is 1.07), the distances di of the crystal planes correspond to the crystal planes of platinum {111}, platinum {200}, platinum {220}, and platinum {311} respectively, and the distances di of the crystal planes correspond to the crystal planes of platinum electron diffraction patterns (PDF # 88-2343). By

The synthesized platinum nanochain is known to have a face-centered cubic structure. The prepared nano material is a polycrystalline platinum nano chain with the particle size of 3 nm. With reference to FIG. 3, the chloroplatinic acid solution has distinct ultraviolet characteristic absorption peaks at 200nm and 260 nm; the ultraviolet characteristic absorption peak at 260nm of the platinum nano-chain solution disappears, which shows that PtCl₆ ^2-Has been completely reduced. And with reference to the attached figure 4, the ultraviolet-visible absorption spectrograms of the prepared platinum nano-chain solution are respectively placed for 0 day, 10 days, 30 days, 50 days, 70 days and 90 days, and the spectral scanning spectrum is not obviously changed within 90 days, which indicates that the prepared platinum nano-chain has good stability.

Example 1

A preparation method of platinum nano-chains comprises the following steps:

(1) putting all glass containers required by the preparation of the platinum nanochain into aqua regia for soaking for 3 hours, then sequentially cleaning the glass containers by using tap water, deionized water and ultrapure water, and drying the glass containers for later use;

(2) adding 25mL of chloroplatinic acid aqueous solution with the mass fraction of 0.01% into a 100mL beaker, stirring and heating at 280 ℃ until the mixture is boiled;

(3) sequentially adding 500uL of 1 mass percent sodium citrate aqueous solution, 250uL of 0.1 mass percent sodium citrate aqueous solution and 250uL of 1 mass percent sodium borohydride aqueous solution into the chloroplatinic acid aqueous solution which is heated to boiling in the step (2), wherein at the moment, the solution is immediately changed from colorless to tawny, heating to boiling at 280 ℃, adjusting the temperature to 100 ℃ and continuously heating for 15min, the solution is changed from tawny to light brown and is not changed, removing a heat source, and then continuously stirring for 10min and cooling to room temperature;

(4) and (4) transferring the solution cooled to room temperature in the 100mL beaker in the step (3) to a 25mL volumetric flask, and carrying out constant volume to scale with ultrapure water to obtain the platinum nano-chain solution.

The above description is an embodiment of the present invention. The embodiments and specific parameters in the embodiments are only for the purpose of clearly illustrating the invention verification process of the inventor and are not intended to limit the scope of the invention, which is defined by the claims, and all equivalent structural changes made by using the contents of the specification and the drawings of the present invention should be covered by the scope of the invention.

Claims (1)

1. A preparation method of a platinum nano-chain is characterized by comprising the following steps:

(1) putting all glass containers required by the preparation of the platinum nanochain into aqua regia for soaking for 3 hours, then sequentially cleaning the glass containers by using tap water, deionized water and ultrapure water, and drying the glass containers for later use;

(2) adding 25mL of chloroplatinic acid aqueous solution with the mass fraction of 0.01% into a 100mL beaker, stirring and heating at 280 ℃ until the mixture is boiled;

(3) sequentially adding 500uL of 1 mass percent sodium citrate aqueous solution, 250uL of 0.1 mass percent sodium citrate aqueous solution and 250uL of 1 mass percent sodium borohydride aqueous solution into the chloroplatinic acid aqueous solution which is heated to boiling in the step (2), wherein at the moment, the solution is immediately changed from colorless to tawny, heating to boiling at 280 ℃, adjusting the temperature to 100 ℃ and continuously heating for 15min, the solution is changed from tawny to light brown and is not changed, removing a heat source, and then continuously stirring for 10min and cooling to room temperature;

(4) and (4) transferring the solution cooled to room temperature in the 100mL beaker in the step (3) to a 25mL volumetric flask, and carrying out constant volume to scale with ultrapure water to obtain the platinum nano-chain solution.

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